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Sodium Thiosulfate → HCID 117974507、化合物

HRID 2272907
ノート
印刷プレビュー

反応式

HRID 2272907 の反応式
Cl[C:2]1C=C(C=C[CH:11]=1)C(OO)=O.C(S[C:15]1[N:16]([C:20]2[N:32]([CH3:33])[C:23]3=[N:24][CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:27]=[C:22]3[N:21]=2)[CH:17]=[CH:18][CH:19]=1)C.[S:34]([O-:38])([O-])(=[O:36])=S.[Na+].[Na+]>C(Cl)(Cl)Cl>[CH2:2]([S:34]([C:15]1[N:16]([C:20]2[N:32]([CH3:33])[C:23]3=[N:24][CH:25]=[C:26]([C:28]([F:31])([F:29])[F:30])[CH:27]=[C:22]3[N:21]=2)[CH:17]=[CH:18][CH:19]=1)(=[O:38])=[O:36])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 117974191HCID 117974191、化合物

生成物 1

HCID 117974507HCID 117974507、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

0.5 g of 3-chloroperoxybenzoic acid (purity of 65% or more) was added to a mixture of 0.32 g of 2-(2-ethylthiopyrrol-1-yl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine and 8 ml of chloroform, under ice cooling, and the mixture was stirred at room temperature for 3 hours and then allowed to stand overnight at room temperature. A 10% aqueous sodium thiosulfate solution was poured to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with a saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulfate, then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.33 g of 2-(2-ethylsulfonylpyrrol-1-yl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (Compound of Present Invention (24)).

後処理

  1. waitto stand overnight at room temperature
  2. extractionthe mixture was extracted with chloroform
  3. washThe organic layer was washed with a saturated aqueous sodium bicarbonate solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2f89a66bffe6492d80c54bd5126eb804
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09120792B2

反応ノート

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